Australian Centre for Research on Separation Science (ACROSS), School of Physical Sciences-Chemistry, University of Tasmania, Hobart, Australia; Materials Chemistry Research Unit, Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen, Thailand.
Electrophoresis. 2014 May;35(10):1478-83. doi: 10.1002/elps.201300512. Epub 2014 Mar 20.
The common SDS microemulsion (i.e. 3.3% SDS, 0.8% octane, and 6.6% butanol) and organic solvents were investigated for the stacking of cationic drugs in capillary zone electrophoresis using a low pH separation electrolyte. The sample was prepared in the acidic microemulsion and a high percentage of organic solvent was included in the electrolyte at anodic end of capillary. The stacking mechanism was similar to micelle to solvent stacking where the micelles were replaced by the microemulsion for the transport of analytes to the organic solvent rich boundary. This boundary is found between the microemulsion and anodic electrolyte. The effective electrophoretic mobility of the cations reversed from the direction of the anode in the microemulsion to the cathode in the boundary. Microemulsion to solvent stacking was successfully achieved with 40% ACN in the anodic electrolyte and hydrodynamic sample injection of 21 s at 1000 mbar (equivalent to 30% of the effective length). The sensitivity enhancement factors in terms of peak height and corrected peak area were 15 to 35 and 21 to 47, respectively. The linearity R(2) in terms of corrected peak area were >0.999. Interday precisions (%RSD, n = 6) were 3.3-4.0% for corrected peak area and 2.0-3.0% for migration time. Application to spiked real sample is also presented.
常用的 SDS 微乳液(即 3.3% SDS、0.8%辛烷和 6.6%丁醇)和有机溶剂被用于研究在使用低 pH 分离电解质的毛细管区带电泳中阳离子药物的堆积。样品在酸性微乳液中制备,并在毛细管的阳极端包含高比例的有机溶剂在电解质中。堆积机制类似于胶束到溶剂堆积,其中胶束被微乳液取代,用于将分析物输送到富含有机溶剂的边界。该边界位于微乳液和阳极电解质之间。阳离子的有效电泳迁移率从微乳液中的阳极方向反转到边界中的阴极方向。通过在阳极电解质中使用 40%的 ACN 和在 1000 mbar 下进行 21 秒的水力样品进样(相当于有效长度的 30%),成功实现了微乳液到溶剂的堆积。以峰高和校正峰面积计的灵敏度增强因子分别为 15 至 35 和 21 至 47。以校正峰面积计的线性度 R(2)大于 0.999。以校正峰面积计的日间精密度(%RSD,n = 6)为 3.3-4.0%,迁移时间的日间精密度为 2.0-3.0%。还介绍了用于加标实际样品的应用。